Trifluoroacetic anhydride → p-Toluenesulfonic acid

HRID 2202833노트

반응식

HRID 2202833 반응식
[CH:1]1([C:4](=O)[CH:5]([N:7]2[CH:12]=[C:11]([I:13])[CH:10]=[CH:9][C:8]2=[N:14][S:15]([C:18]2[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=2)(=[O:17])=[O:16])[CH3:6])[CH2:3][CH2:2]1.FC(F)(F)C(OC(=O)C(F)(F)F)=[O:29]>C1COCC1>[C:21]1([CH3:24])[CH:20]=[CH:19][C:18]([S:15]([OH:16])(=[O:17])=[O:29])=[CH:23][CH:22]=1.[CH:1]1([C:4]2[N:14]=[C:8]3[CH:9]=[CH:10][C:11]([I:13])=[CH:12][N:7]3[C:5]=2[CH3:6])[CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 131735781N-(1-(1-Cyclopropyl-1-oxopropan-2-yl)-5-iodopyridin-2(1H)-ylidene)-4-methylbenzenesulfonamide

생성물 2

HCID 6101p-Toluenesulfonic acidHCID 896903982-Cyclopropyl-6-iodo-3-methylimidazo[1,2-a]pyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of N-(1-(1-cyclopropyl-1-oxopropan-2-yl)-5-iodopyridin-2(1H)-ylidene)-4-methylbenzene sulfonamide (30.5 g) in THF (300 ml) was added trifluoroacetic anhydride (18.3 ml) dropwise. After 3 h, the resulting precipitate was collected by filtration, and washed with ether to give p-toluenesulfonic acid salt of the title compound as a white solid. The solid obtained was dissolved in a mixture of 1 M NaOH, EtOAc and THF. Then the organic layer was washed with brine, dried over MgSO4 and concentrated. The resulting solid was triturated with IPE, and collected to give the title compound (17.7 g) as a pale yellow solid.

후처리

  1. filtrationthe resulting precipitate was collected by filtration
  2. washwashed with ether

출처 및 근거

ORD 기록
ord-938062ca7cf144798bd98ab7d67b0abb
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365540B2

반응 노트

불러오는 중…